Process of dehydrating glauber salt.



No. 685,792. Patented Nov 5, I901.

H. PEMBERTON, In.

PROCESS OF DEHYDRATING GLAUBER SALT. (Application filed Jan. 30, 1901.)

(No Model.) I '2 Sbaets8heei I.

WITNESSES; VENTOR:

3/2231? M??? W 1 M No, 685,792. Patented Nov. 5, I90I.

H. PEMBERTDN, JR. PROCESS OF DEHYDRATJNG GLAUBER SALT.

(Application filed Jan. 80, 1901.)

(No Modem I I 2SheetsSheet 2.

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s a S c WlTNESSES: NVENTOR:

J'Nrrno STnTas PATENT Qfrrrcn.

HENRY PEMBERTON, JR, OF PHILADELPHIA, PENNSYLVANIA.

PROCESS OF DEHYDRATING GLAUBER SALT.

SFIEGIFICATION forming part of Letters Patent No. 685,792, dated November 5, 1901.

A plication filed January 30, 1901. Serial No. 45,283. (No specimens.)

To to whom it may concern:

Be it known that I, HENRY PEMBERTONJr. a citizen of the United States, residing at No. 1008 Clinton street, in Ihecity and county of Philadelphia and State of Pennsylvania, have invented certain new and useful Improvements inProcesses of Dehydrating Crystallized Sodium Sulfate, whereof the following is a specification, reference being had to the accompanying drawings.

Orystallized sodium sulfate, commonly called Glauber salt, when pure contains about fifty-six per cent. water. The salt occurs naturally in large quantities in what are called soda-lakes, where, however, the native crystals contain an increased percentage of water due to mechanical absorption,so that in this state the crystallized salt frequently contains about sixty per cent. of water. The old way of obtaining anhydrous salt from these native crystals was to heat them until they dissolved in their water of crystallization and then evaporate the water by boiling and follow by calcination in a reverberatory furnace. This process consumed a large amount of fuel and time, was constantly interfered with by the tendency during the boiling process of the anhydrous precipitate to cake against the bottom and sides of the vessel, so that it became cracked or burned out, and necessarily resulted in an impure product by reason of the fact that the native crystals are rarely, if ever, perfectly pure, and the process afforded no opportunity for the removal of the impurities.

By Letters Patent of the United States No. 392,286, granted to me November 6, 1888, I patented and described an improved process which consists, essentially, in running a hot saturated solution of sulfate of soda into a vessel containing the crystals until they melt and then allowing the anhydrous salt, or rather such proportion of it as will separate under these conditions, to precipitate and afterward running off the remaining solution or mother-liquor and drying the precipitate. This I found to be a great improvement upon the old processes.

My present process consistsin an improvement upon that which I previously patented in that I maintain a continuous circulation of the hot solution, wherebyl am able to carryon the'precipitating process at a higher temperature, (although still below the boilingpoin-t, )and thereby obtain an increased yield, owing to the fact that the solubility of the anhydrous sulfate decreases as the temperature rises. I also obtain by my improved process a considerable saving of fuel and labor and other accompanying advantages which I 4 is maintained at a temperature less than the boiling-point and yet as near that limit as is practicable by continuously circulating the hot mother-liquor between the two vessels,

so that it can perform its function of effecting thev precipitation of the anhydrous salt from the melted crystals in the one vessel at a temperature near to but below the boilingpoint, while in the other the consequent loss of heat is regained.

I further provide in my present process for the successive use of two or more of those compartments which contain the crystallized salt, so that while precipitation is going on in one the removal of the precipitate can be effected in another. I also employ the excess of hot mother-liquor for the purpose of preheating the crystals which are about to b treated.

In the accompanying drawings I have illustrated two simple forms of apparatus in which to carry on my improved process, itbeing understood, however, that my process is not dependent upon the particular form of apparatus described and that the process may be carried on in any suitable apparatus. I may here remark, however, thatit is essential that any apparatus for the practice of this process, as well as the condition of the process, should be such as to require a minimum expenditure for fuel and labor, because of the fact that the finished product (salt cake) has a commercial value so low that it will not vessel.

ri-I

permit of much expense in handling or of much fuel, as is necessary in'any process which relies upon evaporation merely.

In the accompanying drawings, Figure 1 is a plan view of a suitable apparatus such as I have referred to. 'Fig. 2 is a vertical crosssection of the same along the line 2 2, Fig. 1. Fig. 3 is a vertical longitudinal section of the same along the line 3 3, Fig. 1. Fig. 4 is a plan view of an alternative form of appa-' ratus. Fig. 5 is a vertical cross-section of Fig. 4 along the line 5 5, and Fig. 6 is a vertical longitudinal section or. Fig. 4 along the line 6 6. v

In both the forms of apparatus which I have described the treatment is efiected in a metal vessel the depth of which is comparatively small as related to its other dimensions. I have shown a direct fire for the purpose of applying the heat; but it will be understood that other means for applying heat may be substituted therefor.

Referring to Fig. 1, it will be observed that the apparatus'consists of a large flat rectangular metal vessel or pan A, divided about the middle into two compartments by a partition B. Of the two compartments thusproduced the one to the left (lettered C) is the one.

where the continual heating of the motherliquor occurs. To the right of partition B the vessel is again subdivided by a longitudinal partition D into two compartments E E, both of which are used for the precipitation step of the process. Along the righthand end of the vessel is ashallow trough F, communicating with the compartments E E by suitable openings f f. Partition B has partial openings b b, (see Fig. 2,) cut to about half its depth at each corner, but otherwise is of. the full depth of the vessel. Its central'portion forms a support for a longitu-' dinal trough G, which starts over the center of compartment 0 and runs coincidently with the median line of the vessel to its extreme right-hand end, where it is furnished with two gates g g, opening one over each of the compartments E. Beneath theforward end of compartment 0 is a grate or other fireplace H, the products of combustion being led through a flue running beneath the entire forward end of compartment 0 and in diagonal relation thereto, so that the rotation of the chain continuously lifts liquid from that compartment and delivers it into that end of the trough G. The means for effecting rotation of the endless chain are not shown, but may most conveniently be applied to the shaft carrying the upper sprocket wheel. The trough F is formed with hollow walls and bottom, and theinterior of thejacket thus formed is placed in communication by a pipe is with the bottom of the trough G, the opening of the pipe to the trough being controlled by a suitable cock 7c, the use of which pipe will be hereinafter explain ed.

.salt is introduced and by the application.

An endless chain J with buckets is mounted on two spr'ocket-wheelsjj near the To start the proeess,,the entire vessel A is f filled with mother-liquorthat is. to'say, aff. solution of sodium sulfate, which has been. 7o L heated and has thrown down all of the an-" hydrous sulfate which it will part with. For this purpose a quantity of the crystallized of a gentle heat the crystals arejmeltedin? their water of crystallization. During this process the compartment G is well stirred'andi; raked in order to prevent caking and scaling which would otherwise occur owing to th dense and adhering character of the anhy drous sulfate which is immediately depos ited as a heavy precipitate. When, all of the crystals have disappeared assuch, all of the 7 precipitated salt in compartment 0 is 're moved from the pan bya rake or similar im plement. .It willrbe understood that this is a preliminary operation only and that there after there is no substantial quantity of pre cipitate in the compartment 0. The vessel; 7 being thus filled with mother-liquor, the heat" t from the fire maybe increased until the temperature in compartment 0 is raised to of nearly to the boiling-point, which can now be done without injury to the vessel or without, the necessity of stirring or raking. The crys-.

tals are fed to the apparatus from any con- 7 venient source along the trough F and are 111;

one of the openings finto one of 16.0031! partments E, which are not so hot as com; partment C by reason of their not being-ex posed to the direct heat of the tire." The crys tals which have been introduced soon mel in the mother-liquor and throw down a defi f nite proportion of their contained sulfate of; soda in the form of a precipitatewhich is. variously termed by different authoritiesthe; anhydrous or the monohydrate sulfate of soda. 1 shall use the firstof these terms; As has been stated, it is important for this i 3 step of the process that there should bev nojj actual, boiling of the contents of vcompart ment E, as the thumping and splashing which results from ebullition interferes seriously with the process and caking at the bottom 1 destroys the apparatus. On the other hand, 2 it is important that the temperature should be maintained as high as practicableppro-f vided it is below the boiling-point, because. 7 of the fact that the insolubility. of the an-.",rz'o-1 hydrous salt increases as the temperature; rises, so that the higher the temperature the greater the yield of precipitate. It is not practical to thus regulate the temperature by the direct application of heat, for a fire below the compartment causes caking, and

is set in motion and the hot or boiling liquor delivered to trough G and thence fed continuously into compartment E by the corresponding gate 9. Here it acts upon the crystals, and, mingled with the new mother-liquor produced from the crystals, flows back into compartment 0 through the opening I), Where, however, the unbroken lower half of the par-V.v tition prevents the precipitate from escaping. There is a constant tendency toward a low temperature in compartment E, due to three causes-first, it is impossible, for the reasons explained, to maintain a high temperature by direct heat at the bottom of the vessel; second, the temperature is constantly lowered by the introduction of new supplies of comparatively cold crystals, and, third, the solution or melting of the crystals in the motherliquor is an endothermic action constantly absorbing heat. To overcome these cooling tendencies,the steady and oftentimes rapid circulation of the liquor from the heated compartment O is necessary.

WVithin compartment E there are three more or less distinct layers-first, the motherliquor on top, mingled with that additional quantity which has been yielded by the crystals introduced, which as it cools is constantly flowing back into compartment 0 to be rereheated; below this a slushy mixture of melting crystals, and at the bottom a dense deposit of the separated anhydrous salt,which has a specific-gravity approaching that of sand and lies as a heavy mass resembling mortar or schmierkase at the bottom. It is obvious that as additional crystals are added and melted the total quantity of mother-liquor will be always increasing. In order to prevent this excess from overflowing the edge of the vessel, an outlet is provided in the shape of a pipe 70, through which as rapidly as is necessary some of the liquor is run ofi through the jacket or trough F, where it serves the purpose of keeping the trough hot enough to somewhat raise the temperature of the otherwise cold supply of crystals ready to be introduced into compartment E. After thus yielding its heat the liquor may run 01f into any convenient place (or back into the soda-lake, if convenient) to cool or to evaporate, and thereby form new crystals. As soon as the precipitate in one of the compartments E is formed to the extent of reaching to the height of the bottom of the opening b the use of that compartment is temporarily stopped by closing the gate g, leading from trough G to that compartment, and opening instead that leading to the other compartment E, where a like process of introduction and melting of the orystals',with precipitation, is carried on, during which time the precipitate in the first-used compartment is removed by raking it out onto drainers, where it may afterward be heated in the cal cining-furnace, as described in my previous patent. be resorted to for raking the precipitate into If desired, mechanical means may side pockets, from which it can be removed by an elevator. It will thus be seen that by the alternate use of compartments E E the process as far as the heating of the motherliquor is concerned may be maintained without interruption, and consequently without any waste of heat, a constant stream always being pumped out of O and allowed to be discharged upon a new supply of crystals.

I have spoken of thetemperature at O as being at or near the boiling-point. There is thus a certain amount of evaporation carried on there, although this should not reach the point of violent ebullition. Owing to this fact the mother-liquor is constantly maintained at full strength, and the excess of mechanically-adhering water, which, as 1 have stated, generally accompanies the crystals, is removed. The removal of this excess increases the yield of precipitate. If any precipitation of anhydrous sulfate takes place in compartment 0, it should be from time to time raked out.

It will of course be understood that there is no necessity for limiting the number of compartments E to two, and although I have found the form of apparatus described a convenient one additional compartments may be placed near and in similar communication with compartment 0. Likewise the means for circulating the mother-liquor maybe varied. One such alternative apparatus is shown in the drawings in Figs. 4,5, and 6, where the circulation is maintained without raising the liquor to the higher level. In this'arrangement compartment 0 contains two sluices c 0, formed at either side and running to near the left-hand extremity. Partition B is formed with a central gate 1), as well as two side gates b b,which communicate with the sluices. Partition D, between the compartments E E, is movable and may be placed at one side or the other, so as to throw gate 1) into communication with either one or the other of the compartments E. In compartment 0, immediately opposite the gateway b, is a paddle- Wheel G, mounted on a shaft just above the level of the liquor and continuously revolving, with its lower paddles immersed therein, so as to force the mother-liquor through the IIO gate 5' into one or other of the compartments E,whence after circulating therethrough and melting the crystals which are being introduced there from trough F it returns through one of the sluieeways to the other end of the compartment 0 and is again heated. A fallpipe L is used to remove the excess of motherliquor.

It will be seen that whatever apparatus is used this process possesses a number of advantages on account of its being continuous in its action and to a degree automatic. As contrasted with an intermittent method of treatment there is a saving of fuel, because there is no drawing of fires 'nor loss of heat in cooling and reheating the apparatus when this is being emptied and recharged.- As

- hold them in solution there.

there are no stoppages in the operation, the

output is greater, and there is therefore a corresponding lessening of the cost of labor per ton of finished salt cake. As contrasted with the old-time plan of boiling down directly to a mush, there is no caking of the thick mass on the containing vessel, with the consequent cracking or burning out of the same. The smoke and fire-gases do not come in contact with the liquor or crystals and the product yielded is white and not discolored. Consequently there is a decided saving of both time and coal in the subsequent treatment in the calcining-furnace. The mass in the furnace simply has to be heated until the water is driven off and does not have to be calcined to redness in order to burn ofi the ahering carbon derived from the smoke. Under the old method the mass had to be stirred for two or three hours at a full red heat in the furnace to burn it white, whereas by my present process it is necessary to heat it for only thirty to forty-five minutes in the furnace to drive off the water. This process also possessess the additional advantage of yielding a pure product. Many of the native soda de posits contain some admixture of the salts of magnesium and also of the salts of sodium other than the sulfate-for example, the chlorid, borate, and one or more of the several carbonates of sodium. The borate and the carbonates have a higher commercial value than the sulfate. The greater portion of all of the above-mentioned salts is separated from the anhydrous sulfate (that falls down) and passes out in the mother-liquid, provided these salts do not occur in too large a percentage and provided that the temperature of the mother-liquor in the precipitating-compartment be maintained sufficiently high to The circulatory system of my process is peculiarly adapted to accomplishing this end.- As a result the anadmixed salts, and these salts are obtained in a more concentrated form in the motherliquor-a' condition more favorable to their subsequent recovery than exists when other processes are used.

The entire plant is simple and is peculiarly adapted to handling the crystals in situ in the event of the operation being carried out at the deposits where the soda salts occur. It is precisely in such remote regions that a process free from wear andrte ar and from complicated apparatus is desirable. Thisis more especially truewhen, as in this case, the resulting product hasalow commercial value.

Having thus described my invention, 1 claim- 7 1. The process of extracting anhydrous sulfate of soda from Glauber salt in admixture ,with other salts, which consists in continuously treating the salts in one compartment with a hot saturated solutionof'sulfate of soda until they'melt and precipitate the anhydrous sulfate; continuously heating the anhydrous sulfate and calcining it, substan solution up to or near the boiling-point inanother compartment; continuously causing the solution to circulate between the two con1 7. partments removing from the apparatus the V excess of solution supplied by the melting of; g 5 the new salts and containing in solution the admixed salts; and removing the precipitated V tially as described. '.i 1 2. The process of dehydrating Glauber salt, which consists in treating the crystals in'one compartment with a hot saturated solutionof 1 r sulfate of soda until they melt and precipitate 8o the anhydrous sulfate; heating the solution 7' up to or near the boiling-point in another compartment; and causing the solution to circu- 1 late continuously between the two compartments, substantially as described. 7 p

3. The process of dehydrating Glauber salt, which consists in treating the crystals in one *compartment with a hot saturated solution of 7;; t;

sulfate of soda until they melt and precipij V tate the anhydrous sulfate; heating the solution in another compartment to the point of gentle ebullition, whereby the excess of water contained in the native crystals is remove'dg; by evaporation; and causing the solutionto 7 1 circulate continuously between the two com-' 9; partments, substantially as described. at. The process of dehydrating Glauber salt, 7 I;- which consists in treating the crystals in one I if compartment with a hot saturated solution of r sulfate of soda until they melt and precipi-fi oo' tate the anhydrous-sulfate; heating the solu J tion up to or near the boiling-point in an: other compartment; continuously causing 1]} thesolution to circulate between the two c0m-; y partments and removing from the apparatus: res: the excess of solution supplied by the melting of the new crystals,substantially asdescribed 5. The process of dehydrating Glaubersalt, which consists inr treating the crystals in one-i compartment with a hot saturated solutionofe rio sulfate of soda until they melt and precipi-f 1 tate the anhydrous sulfate; continuously heating the solution up to or near the boiling Q point in another compartment; continuously causing the'solution to circulate between the two compartments; removing'from theapparatus the excess of solution supplied byrthe melting of the new crystals; and utilizing I this heated excess of solution caused by the melting of the new crystals to partially pre-j heat the supply of crystals about to be intro from those of the precipitating-compartments through which for the time being the circulation is not maintained, substantially as described.

7. The process of dehydrating Glauber salt, which consists in continuously introducing into the compartment containing it a solution of sulfate of soda, at atemperature at or near I the boiling-point, and continuously Withdrawing the same, whereby a maximum amount 10 of the anhydrous salt is precipitated, substantially as described.

HENRY PEMBERTON, JR. Witnesses: v

JAMES H. BELL, E. REESE. 

